Method and device for preparing 2,5-furandicarboxylic acid by combined technology of microwave-induced strengthening and azeotropic distillation

Abstract

The invention discloses a method and a device for preparing 2,5-furandicarboxylic acid by the combined technology of microwave induction strengthening and constant boiling rectification water removal. The device organically combines microwave-induced strengthening and azeotropic distillation to remove water. The steps of the method are as follows: 1) open the reaction kettle and stir, add sulfolane, hexanedioic acid (salt), sulfuric acid, petroleum ether, and wave absorbing agent to the reaction kettle in turn, turn on the microwave oven and the temperature control system, and set the temperature at 95 to 120° C. The reaction is continued for 0.5~3 h, and the water produced by the reaction and the petroleum ether form an azeotrope and slip out from the top of the tower; 2) After the reaction is completed, cool down, release the reaction liquid, filter out the absorber for reuse, and the filtrate is neutralized by alkali, reduced The sulfolane is recovered by pressure distillation, and the 2,5-furandicarboxylic acid product is obtained after crystallization and recrystallization. The invention greatly reduces the reaction time required for preparing 2,5-furandicarboxylic acid through dehydration and cyclization of hexanedioic acid (salt) by inducing coupled microwave strengthening through the wave absorbing agent, thereby greatly improving the space-time yield thereof.

Description

technical field [0001] The invention belongs to the field of process strengthening in the chemical industry, and particularly relates to a method and a device for preparing 2,5-furandicarboxylic acid by the combined technology of microwave induction strengthening and azeotropic distillation for water removal. Background technique [0002] With the increasing uncertainty of fossil resources and the strengthening of people's awareness of environmental protection, renewable biomass as a raw material for chemical industry has attracted more and more attention. Among them, biomass-based 2,5-furandicarboxylic acid (2,5-Furandicarboxylic acid, abbreviation: 2,5-FDCA, CAS number: 3238-40-2) is similar in structure to petroleum-based terephthalic acid. Polymers, pharmaceuticals, fine chemicals, solvents and other fields have broad application prospects. In 2004, it was listed as one of the twelve biomass-based platform compounds by the US Department of Energy (Werpy T, Petersen G. To...

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Problems solved by technology

But the reaction time required by this patent is very long (15~48h), and the space-time yield (Space-Time Yield) of unit volume reactor is very low

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